CN106588862A - Ethylene carbonate purification process and purification system - Google Patents
Ethylene carbonate purification process and purification system Download PDFInfo
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- CN106588862A CN106588862A CN201611104582.3A CN201611104582A CN106588862A CN 106588862 A CN106588862 A CN 106588862A CN 201611104582 A CN201611104582 A CN 201611104582A CN 106588862 A CN106588862 A CN 106588862A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D317/00—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms
- C07D317/08—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3
- C07D317/10—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings
- C07D317/32—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D317/34—Oxygen atoms
- C07D317/36—Alkylene carbonates; Substituted alkylene carbonates
- C07D317/38—Ethylene carbonate
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Abstract
The invention provides an ethylene carbonate purification process, wherein the purification process comprises the following steps: firstly, an ethylene carbonate crude product is sent into a continuous rectification process, light component impurities are removed at a top, heavy component impurities are removed at a bottom, and an ethylene carbonate intermediate purified product is extracted from a side line; then the ethylene carbonate intermediate purified product obtained in the former step is buffered and then is sent into an intermittent rectification process, gas-liquid balance is established after heating, then a light component substance is removed at the top, and the ethylene carbonate product is extracted from the side line. The crude ethylene carbonate material is refined by a continuous rectification tower, the light component impurities and the heavy component impurities are extracted from the tower top and the tower bottom respectively, and the ethylene carbonate material is extracted from the side line, then enters the intermittent rectification tower and is further refined; after the light component impurities are extracted from the tower top of the intermittent rectification tower, and finally the ethylene carbonate product is extracted from the side line; moreover, various indicators fully meet the indicator requirements of application of a lithium ion battery electrolyte solution solvent.
Description
Technical field
The present invention relates to ethylene carbonate purification technique field, is related to a kind of ethylene carbonate purifying technique and purification system
System, more particularly to a kind of highly purified ethylene carbonate purifying technique and purification system.
Background technology
Ethylene carbonate, also known as DOX -2- ketone, molecular formula is C3H4O3, abbreviation EC is a kind of function admirable
Organic solvent, multiple polymers can be dissolved, with many excellent performances.Which can substitute epoxy second as organic intermediate
Alkane is used for dioxy glycosylation reaction, or the primary raw material of dimethyl carbonate production by transesterification, and can also act as synthesizing furan
The raw material of oxazolone, waterglass system slurry, fibre trimmer etc., also act as production lubricating oil and grease in the industrial production
Reactive intermediate.
Especially in recent years, highly purified ethylene carbonate is also mainly used in lithium battery electrolytes.It is lithium battery
The maximum solvent of consumption in liquid, and future are solved with the development of Soft Roll electrokinetic cell, the consumption of ethylene carbonate ester solvent can be more next
Bigger, development prospect is wide, but the naturally also more and more higher therewith of the requirement to product quality.
The preparation of ethylene carbonate mainly has phosgenation, ester-interchange method and oxirane and carbon dioxide addition process.Wherein,
Phosgenation is the method for earliest preparation of industrialization ethylene carbonate, as phosgene has severe toxicity and produces serious pollution to environment,
It is prohibited from using in many countries；Ester-interchange method is to prepare ethylene by the ester exchange reaction of diethyl carbonate and ethylene glycol
The method of alkene ester is exactly ester-interchange method, but yield is not high, and there is a problem of that cost of material is high and catalyst efficiency is low, institute
It is worth with practical application in industry not high.
Thus, at present in the commercial production of country's ethylene carbonate, main still oxirane and carbon dioxide addition process.
Synthesis reactor by oxirane and carbon dioxide additive reaction synthesizing ethylene carbonate crude product, is then divided by the method first again
The thick ethylene carbonate material for separating out obtains highly purified ethylene carbonate product after purification.
But existing purifying technique, different degrees of deposit high energy consumption, operative's high labor intensive.The purity of extraction material
Low, product yield is low and the problems such as unstable product quality.Especially purity is generally only capable of reaching 99.95% or so, and this is right
For the LITHIUM BATTERY product quality indicator of electrolyte solvent, also with a certain distance.
Therefore, how a kind of purifying technique of ethylene carbonate is provided, can be further improved ethylene carbonate purity, be obtained
To highly purified ethylene carbonate, it has also become one of focus of many line scientific research personnel's extensive concerns in field.
The content of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of ethylene carbonate purifying technique and deduction system
System, particularly a kind of highly purified ethylene carbonate purifying technique and deduction system, the purifying technique purification that the present invention is provided
Ethylene carbonate, product purity can reach more than 99.99%, and indices fully meet lithium-ion battery electrolytes solvent should
Index request.
The invention provides a kind of ethylene carbonate purifying technique, comprises the following steps：
1) ethylene carbonate crude product is sent into into continuous rectificating technique, top removing light component impurity, bottom removing heavy constituent
Impurity, side take-off ethylene carbonate intermediate purification product；
2), after the ethylene carbonate intermediate purification product that obtain above-mentioned steps are buffered, batch fractionating technique, heating are sent into
Set up removing light component material in top after vapor liquid equilibrium, side take-off ethylene carbonate product.
Preferably, the step 1) in, the operating pressure at the top is 1～5KPa, and the operation temperature at the top is
130～150 DEG C；The operating pressure of the bottom is 5～20KPa, and the operation temperature of the bottom is 135～165 DEG C；
The step 2) in, the operating pressure at the top is 1～5KPa, and the operation temperature at the top is 130～150
℃；The operating pressure of the bottom is 5～20KPa, and the operation temperature of the bottom is 135～170 DEG C.
Preferably, the purity of the ethylene carbonate crude product is 99.5%～99.8%；
The purity of the ethylene carbonate intermediate purification product is 99.9%～99.98%.
Preferably, the step 1) in, the top removing light component impurity is specially top carries out condensing reflux removing
Light component impurity；
The reflux ratio of the backflow is 20～80；
The produced quantity of the light component impurity is 0.1～0.4 with the ratio of the inlet amount of the ethylene carbonate crude product；
The bottom removing heavy constituent impurity is specially bottom and is boiled circularly removing heavy constituent impurity again；
The produced quantity of the heavy constituent impurity is 0.1～0.4 with the ratio of the inlet amount of the ethylene carbonate crude product.
Preferably, the step 2) it is specially：
21), after the ethylene carbonate intermediate purification product that obtain above-mentioned steps are buffered, send into batch fractionating technique；
22), after vapor liquid equilibrium is set up in heating, top carries out total reflux operation, and bottom is boiled extinction recycle operation again；
23) at the top of, light component material collection removes light component material to after finite concentration, first, and side line starts to produce carbonic acid again
Vinyl acetate product；
24) ethylene carbonate product discharges bottom heavy constituent residual liquid less than extraction ethylene carbonate after standard, is stopped；
25) circulation step 22)～24).
Preferably, the step 23) in, after the side line starts to produce ethylene carbonate product, it is gradually reduced top light
The removing amount of component materials.
Preferably, the vapor liquid equilibrium has distillation for top with reference to condition, begins with backflow；
The temperature of the heating is 130～160 DEG C；
The time of the total reflux operation is 1～5 hour；
The time for first removing light component material is 0.5～3 hour；
The removing amount of the light component material is 0.1～0.3 with the ratio of the inlet amount for sending into batch fractionating technique.
Preferably, the light component material collection to finite concentration be light component content in 0.1～2wt%；
The standard of the ethylene carbonate product includes the total content of purity, colourity, ethylene glycol and diethylene glycol and aqueous
One or more in amount.
Preferably, it is characterised in that the purity of the ethylene carbonate product is more than or equal to 99.99%；
The colourity of the ethylene carbonate product is less than or equal to 5；
The total content of the ethylene glycol and diethylene glycol of the ethylene carbonate product is less than or equal to 30ppm；
The water content of the ethylene carbonate product is less than or equal to 20ppm.
Present invention also offers a kind of ethylene carbonate purification system, including：Continuous rectifying tower, continuous rectification column overhead are cold
Condenser, continuous rectifying tower overhead reflux device, continuous rectifying tower tower reactor reboiler, batch fractionating tower feeding buffer device, interval
Rectifying column, batch fractionating tower overhead condenser, batch fractionating tower overhead reflux device and batch fractionating tower tower reactor reboiler；
Described continuous rectifying tower overhead condenser one end is connected with continuous rectifying tower top gaseous phase outlet, the other end
It is connected with the continuous rectifying tower overhead reflux device, the continuous rectifying tower overhead reflux device and the continuous rectifying tower
Tower top fluid inlet is connected；
Described continuous rectifying tower tower reactor reboiler one end is connected with the continuous rectifying tower tower reactor liquid-phase outlet, the other end
It is connected with the continuous rectifying tower tower reactor gas phase import；
Described batch fractionating tower feeding buffer device one end is connected with the continuous rectifying tower survey line products export, another
End is connected with the batch fractionating tower charging aperture；
Described batch fractionating tower overhead condenser one end is connected with batch fractionating tower top gaseous phase outlet, the other end
It is connected with the batch fractionating tower overhead reflux device, the batch fractionating tower overhead reflux device and the batch fractionating tower
Tower top fluid inlet is connected；
Described batch fractionating tower tower reactor reboiler one end is connected with the continuous tower bottom of rectifying tower liquid-phase outlet of the interval, another
End is connected with the batch fractionating tower tower reactor gas phase import.
The invention provides a kind of ethylene carbonate purifying technique, comprises the following steps, first by ethylene carbonate crude product
Send into continuous rectificating technique, top removing light component impurity, bottom removing heavy constituent impurity, in the middle of side take-off ethylene carbonate
Purification product；Then, after the ethylene carbonate intermediate purification product that above-mentioned steps obtained are buffered, batch fractionating technique, heating are sent into
After set up top removing light component material, side take-off ethylene carbonate product after vapor liquid equilibrium.Compared with prior art, this
It is bright for traditional high purity carbon vinyl acetate method of purification, by thick ethylene carbonate material through multi-stage batch distillation operation,
Purification obtains highly purified ethylene carbonate product, after batch fractionating tower operation takes tower top first to produce light component material, tower top
The mode of operation of high purity carbon vinyl acetate product is produced again, and batch fractionating is also performed to total reflux operation, thus there is technique
Complexity, high energy consumption, the high labor intensive of operative, the purity of overhead extraction material are low, produce product yield is low, product matter
Measure the problems such as unstable.
The present invention can not be used in purification in the cyclic carbonate for overcoming industrialized production present in prior art
On the basis of the technology prejudice of continuous rectification operation, combined using continuous rectification operation and batch fractionating operation, carried overall
Creative Design is carried out in pure technique, by thick ethylene carbonate material, refined through continuous treating tower, tower top, bottom of towe are adopted respectively
Go out weight composition impurity, side take-off ethylene carbonate material enters back into batch fractionating tower and further refines, batch fractionating tower tower
After top extraction light component impurity, finally in side take-off ethylene carbonate product.Test result indicate that, the carbon after present invention purification
Vinyl acetate, purity are higher than 99.99%, and aqueous less than 20ppm, colourity is less than 5, and ethylene glycol and diethylene glycol total content are less than
30ppm, indices fully meet the index request of lithium-ion battery electrolytes solvent application.
Description of the drawings
The technological process sketch plan of the ethylene carbonate purifying technique that Fig. 1 is provided for the present invention.
Specific embodiment
In order to further appreciate that the present invention, the preferred embodiments of the invention are described with reference to embodiment, but
It is it should be appreciated that these descriptions are simply to further illustrate the features and advantages of the present invention rather than to patent requirements of the present invention
Limit.
The all raw materials of the present invention, originate to which and are not particularly limited, commercially buying or according to people in the art
Known to member prepared by conventional method.
The present invention is raw materials used, its purity is not particularly limited, present invention preferably employs ethylene carbonate production technology
Conventional coarse fodder purity.
Device therefor of the present invention, defines to which and is not particularly limited, with the conventional definition in this area.
The invention provides a kind of ethylene carbonate purifying technique, it is characterised in that comprise the following steps：
1) ethylene carbonate crude product is sent into into continuous rectificating technique, top removing light component impurity, bottom removing heavy constituent
Impurity, side take-off ethylene carbonate intermediate purification product；
2), after the ethylene carbonate intermediate purification product that obtain above-mentioned steps are buffered, batch fractionating technique, heating are sent into
After set up top removing light component material, side take-off ethylene carbonate product after vapor liquid equilibrium.
Ethylene carbonate crude product is sent into continuous rectificating technique by the present invention first, and top removing light component impurity, bottom are de-
Except heavy constituent impurity, side take-off ethylene carbonate intermediate purification product.
The present invention is not particularly limited to the source of the ethylene carbonate crude product, with system well known to those skilled in the art
Preparation Method is prepared or commercially available purchase, and those skilled in the art can be according to practical condition, raw material condition and product
Requirement is selected and is adjusted, and the preparation source of ethylene carbonate crude product of the present invention preferably adopts oxirane and titanium dioxide
Thick ethylene carbonate of the carbon for Material synthesis, more preferably thick ethylene carbonate of the purity equal to or higher than 99.5%, most preferably
It is the thick ethylene carbonate equal to or higher than 99.5% for adopting oxirane and carbon dioxide for Material synthesis, wherein described pure
Degree is preferably 99.5%～99.8%, more preferably 99.55%～99.75%, most preferably 99.6%～99.7%.
The present invention is not particularly limited to the continuous rectificating technique, with continuous rectifying tower well known to those skilled in the art
Rectification, those skilled in the art can be selected and be adjusted according to practical condition, raw material condition and product requirement
Whole, the present invention further improves ethylene to overcome existing ethylene carbonate purification use the defect of continuous rectificating technique
The purity of alkene ester product, in the continuous rectificating technique, top removing light component impurity, bottom removing heavy constituent impurity, side line
Extraction ethylene carbonate intermediate purification product, more preferably side entry feed, top removing light component impurity, bottom removing heavy constituent are miscellaneous
Matter, side take-off ethylene carbonate intermediate purification product.
The present invention is not particularly limited to the operating parameter of the continuous rectificating technique, and those skilled in the art can basis
Practical condition, raw material condition and product requirement are selected and are adjusted, in continuous rectificating technique of the present invention, described
The operating pressure at top, i.e., the operating pressure of described continuous rectification column overhead are preferably 1～5KPa, more preferably 2～4KPa, most
Preferably 2.5～3.5KPa；The operation temperature at the top, i.e., the operation temperature of described continuous rectification column overhead are preferably 130
～150 DEG C, more preferably 137～147 DEG C, most preferably 134～143 DEG C；The operating pressure of the bottom, i.e., described continuous fine
The operating pressure for evaporating tower bottom of towe is preferably 5～20KPa, most preferably more preferably 8～17KPa, 10～15KPa；The bottom
Operation temperature, i.e., the operation temperature of described continuous rectifying tower bottom of towe is preferably 135～165 DEG C, more preferably 140～160 DEG C,
Most preferably 145～155 DEG C.
The present invention is not particularly limited to the concrete steps that the top removes light component impurity, with those skilled in the art
Well known routine operation, those skilled in the art can enter according to practical condition, raw material condition and product requirement
Row is selected and is adjusted, and removing light component impurity in top of the present invention is particularly preferred as top and carries out condensing reflux removing light component
Impurity；The present invention is not particularly limited to the reflux ratio of the condensing reflux, with reflux ratio well known to those skilled in the art is
Can, those skilled in the art can be selected and be adjusted according to practical condition, raw material condition and product requirement, this
The reflux ratio of the bright backflow is preferably 20～80, more preferably 30～70, most preferably 40～60.The present invention is to described light group
The produced quantity of impurity is divided to be not particularly limited, with produced quantity well known to those skilled in the art, those skilled in the art can
To be selected and be adjusted according to practical condition, raw material condition and product requirement, light component impurity of the present invention
Produced quantity is preferably 0.1～0.4, more preferably 0.15～0.35 with the ratio of the inlet amount of the ethylene carbonate crude product, most
Preferably 0.2～0.3.
The present invention is not particularly limited to the concrete steps that the bottom removes heavy constituent impurity, with those skilled in the art
Well known routine operation, those skilled in the art can enter according to practical condition, raw material condition and product requirement
Row is selected and is adjusted, and removing heavy constituent impurity in bottom of the present invention is particularly preferred as bottom and is boiled circularly removing heavy constituent again
Impurity；The present invention is not particularly limited to the produced quantity of the heavy constituent impurity, with produced quantity well known to those skilled in the art
, those skilled in the art can be selected and be adjusted according to practical condition, raw material condition and product requirement, this
The ratio of the produced quantity and the inlet amount of the ethylene carbonate crude product of inventing the heavy constituent impurity is preferably 0.1～0.4, more
Preferably 0.15～0.35, most preferably 0.2～0.3.
The present invention is not particularly limited to the extraction ethylene carbonate intermediate purification product, and those skilled in the art can be with root
Selected and adjusted according to practical condition, raw material condition and product requirement, carried in the middle of ethylene carbonate of the present invention
The purity of sterling preferably greater than equal to 99.9%, more preferably 99.91%～99.98%, more preferably 99.93%～
99.96%, most preferably 99.94%～99.95%.
Step 1 of the present invention) can also be specially：
Come from ethylene carbonate synthesis technique and isolate ethylene carbonate crude product of the purity of catalyst higher than 99.5%
Into continuous rectifying tower, removed overhead light component impurity, tower reactor removing heavy constituent impurity, side take-off purity higher than 99.9% with
On ethylene carbonate material.Ethylene carbonate continuous rectifying tower takes negative-pressure operation, the control of tower top operating pressure 1～
5KPa, tower reactor operating pressure are controlled in 5～20KPa；Ethylene carbonate continuous rectification column overhead operation temperature is 130～150 DEG C,
Tower reactor operation temperature is 135～165 DEG C.
The present invention is not particularly limited to the equipment of the continuous rectificating technique, with well known to those skilled in the art continuous
Rectifying column, those skilled in the art can be selected according to practical condition, raw material condition and product requirement and
Adjustment, refining effect of the present invention for further raising continuous rectificating technique, continuous rectifying tower of the present invention are preferably board-like
Tower or packed tower, more preferably packed tower.
The present invention is not particularly limited to the tower plate structure of the plate column, with plate column well known to those skilled in the art
Tower plate structure, those skilled in the art can be selected according to practical condition, raw material condition and product requirement
Select and adjust, tower plate structure of the present invention preferably includes bubble column, sieve-plate tower, valve tower or tongue shape tower.The present invention is to described
The form of bio-carrier of packed tower is not particularly limited, with the form of bio-carrier of packed tower well known to those skilled in the art, ability
Field technique personnel can be selected and be adjusted according to practical condition, raw material condition and product requirement, of the present invention
The form of bio-carrier of packed tower preferably includes structured packing or random packing, and more specifically preferably wire mesh packing, porcelain ripple are filled out
Material, metal corrugated packing, wooden-grid packing, Raschig ring, Pall ring, cascade ring, helical ring, ceramic ring, steel fill out circle, saddle type expect,
Quartz or glass spring, the present invention are the refining effect for further improving continuous rectificating technique, set with other of continuous rectifying tower
Phase matched combined is put, the continuous rectifying tower is preferably packed tower, more preferably wire mesh packing tower, most preferably rustless steel
Wire packing tower.
The present invention is not particularly limited to the parameter of the continuous rectificating technique, with well known to those skilled in the art continuous
Rectification process parameter, those skilled in the art can be carried out according to practical condition, raw material condition and product requirement
Select and adjust, refining effect of the present invention for further raising continuous rectificating technique, the tower of continuous rectifying tower of the present invention
Plate number is preferably 30～60 pieces, more preferably 35～55 pieces, most preferably 40～50 pieces, is particularly preferred as 40 pieces；Institute of the present invention
The number of plates for stating ethylene carbonate crude product side entry feed is preferably the 25th～35th piece, more preferably the 27th～33rd piece, optimum
Elect the 29th～31st piece as, be particularly preferred as the 31st piece；The side take-off number of plates of the present invention is preferably the 5th～15th piece,
More preferably the 7th～13rd piece, most preferably the 9th～11st piece, it is particularly preferred as the 11st piece.
Sequence of the present invention to the column plate is not particularly limited, and knows conventional sort method with those skilled in the art
, i.e., it is the 1st block of column plate at tower top, is last 1 block of column plate at tower reactor.
Instant invention overcomes the cyclic carbonate of industrialized production present in prior art, can not be using company in purification
On the basis of the technology prejudice of continuous distillation operation, operated to ethylene carbonate crude product using continuous rectification, especially with epoxy
Ethane and carbon dioxide first carry out continuous rectification, Jing Guolian for the thick ethylene carbonate equal to or higher than 99.5% of Material synthesis
Continuous treating column is refined, and tower top, bottom of towe produce weight composition impurity respectively, by controlling feed entrance point, unloading position, tower top and tower
Multiple design parameters such as bottom, carry out the selection and combination of creativeness, and final side take-off obtains carbonic acid of the purity higher than 99.9%
Vinyl acetate intermediate purification product, need to carry out multiple batch fractionating purification in effectively solving prior art, can just obtain high-purity
The ethylene carbonate product of degree, and process energy consumption is high, the low problem of stability difference and purity.
After the present invention and then the ethylene carbonate intermediate purification product for obtaining above-mentioned steps are buffered, batch fractionating work is sent into
Skill, sets up removing light component material in top after vapor liquid equilibrium, side take-off ethylene carbonate product after heating.
The present invention is not particularly limited to the concrete mode of the buffering, and those skilled in the art can be according to actual production
Situation, raw material condition and product requirement are selected and are adjusted, and buffering of the present invention is carried out preferably by buffer unit
Buffering, more preferably enters row buffering by surge tank.
The present invention is not particularly limited to the batch fractionating technique, with batch fractionating tower well known to those skilled in the art
Rectification, those skilled in the art can be selected and be adjusted according to practical condition, raw material condition and product requirement
Whole, the present invention can further improve the purity of ethylene carbonate product, the batch fractionating again to reduce the number of times of batch fractionating
In technique, removing light component material in top after vapor liquid equilibrium, more preferably side take-off ethylene carbonate product, bottom are set up in heating
Portion feeds, after vapor liquid equilibrium is set up in heating, top removing light component impurity, and side take-off ethylene carbonate product.
The present invention is not particularly limited to the operating parameter of the batch fractionating technique, and those skilled in the art can basis
Practical condition, raw material condition and product requirement are selected and are adjusted, continuous rectification work of the present invention for cooperation above
Skill, improves the globality of technique, in the batch fractionating technique, the operating pressure at the top, i.e., and described batch fractionating tower tower
The operating pressure on top is preferably 1～5KPa, most preferably more preferably 2～4KPa, 2.5～3.5KPa；The operation at the top
Temperature, i.e., the operation temperature of described batch fractionating column overhead are preferably 130～150 DEG C, more preferably 137～147 DEG C, most preferably
For 134～143 DEG C；The operating pressure of the bottom, i.e., the operating pressure of described batch fractionating tower bottom of towe are preferably 5～20KPa,
More preferably 8～17KPa, most preferably 10～15KPa；The operation temperature of the bottom, i.e., described batch fractionating tower bottom of towe
Operation temperature is preferably 135～170 DEG C, more preferably 140～165 DEG C, most preferably 145～160 DEG C.
Concrete steps of the present invention to the batch fractionating technique, i.e. above-mentioned steps detailed process 2) are not especially limited
System, the step of with batch fractionating technique well known to those skilled in the art, those skilled in the art can be according to actual life
Product situation, raw material condition and product requirement are selected and are adjusted, and the present invention is improved to coordinate continuous rectificating technique above
The globality of technique, the step 2) it is specially：
21), after the ethylene carbonate intermediate purification product that obtain above-mentioned steps are buffered, send into batch fractionating technique；
22), after vapor liquid equilibrium is set up in heating, top carries out total reflux operation, and bottom is boiled extinction recycle operation again；
23) at the top of, light component material collection removes light component material to after finite concentration, first, and side line starts to produce carbonic acid again
Vinyl acetate product；
24) ethylene carbonate product discharges bottom heavy constituent residual liquid less than extraction ethylene carbonate after standard, is stopped；
25) circulation step 22)～24).
The present invention is not particularly limited to the condition of the vapor liquid equilibrium, with batch fractionating well known to those skilled in the art
The condition of the conventional vapor liquid equilibrium of technique, those skilled in the art can according to practical condition, raw material condition and
Product requirement is selected and is adjusted, vapor liquid equilibrium of the present invention with reference to condition be preferably top have distillation, i.e., top
When backflow begins with backflow；Now, preferably regard batch fractionating tower as and reach vapor liquid equilibrium.
The present invention is not particularly limited to the temperature of the heating, with batch fractionating technique well known to those skilled in the art
Temperature in conventional tower, those skilled in the art can be entered according to practical condition, raw material condition and product requirement
Row is selected and is adjusted, and the temperature of heating of the present invention, the i.e. operation temperature of batch fractionating tower tower body are preferably 130～160 DEG C,
More preferably 135～155 DEG C, most preferably 140～150 DEG C.
The present invention was not particularly limited to the concrete time of the total reflux operation, and those skilled in the art can be according to reality
The border condition of production, raw material condition and product requirement are selected and are adjusted, and the time of total reflux operation of the present invention is preferred
For 1～5 hour, more preferably 1.5～4.5 hours, more preferably 2～4 hours, most preferably 2.5～3.5 hours.
Concrete time of the present invention to the total reflux operation, and the concrete time of extinction recycle operation is boiled again without special
Limit, those skilled in the art can be selected and be adjusted according to practical condition, raw material condition and product requirement, this
Invent preferably 1～5 hour time of the total reflux operation, more preferably 1.5～4.5 hours, more preferably 2～4 hours,
Most preferably 2.5～3.5 hours.
The present invention improves the globality of technique, further improves batch distillation to coordinate continuous rectificating technique above
The refining effect of technique, the step 23) in, after the side line starts to produce ethylene carbonate product, it is gradually reduced top light
The removing amount of component materials.The present invention is not particularly limited to the concrete operation step being gradually reduced, with art technology
The routine operation being gradually reduced in technological operation known to personnel, those skilled in the art can be according to actual production feelings
Condition, raw material condition and product requirement are selected and are adjusted.
The present invention is not particularly limited to the concrete steps for first removing light component material, ripe with those skilled in the art
The routine operation known, those skilled in the art can be carried out according to practical condition, raw material condition and product requirement
Select and adjust；The present invention is not particularly limited to the concrete operations parameter for first removing light component material, with this area skill
Conventional parameter known to art personnel, those skilled in the art can be according to practical condition, raw material condition and products
Requirement is selected and is adjusted, preferably 0.5～3 hour time for first removing light component material of the present invention, and more preferably 1
～2.5 hours, most preferably 1.5～2 hours.The present invention is first removed in light component material to described, the removing of light component material
Amount is not particularly limited, and with produced quantity well known to those skilled in the art, those skilled in the art can be according to actual life
Product situation, raw material condition and product requirement are selected and are adjusted, the removing amount of light component material of the present invention with it is described
The ratio for sending into the inlet amount of batch fractionating technique is preferably 0.1～0.3, more preferably 0.13～0.28, most preferably 0.15
～0.25.
The present invention is not particularly limited to the certain density concrete numerical value, with interval well known to those skilled in the art
The enriched concentration of the conventional light component of rectifying tower top, those skilled in the art can be according to practical condition, raw material feelings
Condition and product requirement are selected and are adjusted, finite concentration of the present invention preferably 0.1～2wt%, more preferably 0.3～
1.7wt%, more preferably 0.5～1.5wt%, most preferably 0.7～1.2wt%.
Purity requirement of the present invention to the ethylene carbonate product is not particularly limited, and is known with those skilled in the art
High-purity ethylene carbonate product purity requirement, or meet the purity requirement of LITHIUM BATTERY ethylene carbonate, ability
Field technique personnel can be selected and be adjusted according to practical situations, raw material condition and product requirement, of the present invention
The standard of ethylene carbonate product preferably includes in the total content and water content of purity, colourity, ethylene glycol and diethylene glycol
Plant or various, more preferably the total content and water content of purity, colourity, ethylene glycol and diethylene glycol.Ethylene of the present invention
The specific standards of alkene ester product are preferably, and the purity of the ethylene carbonate product is more than or equal to 99.99%, more preferably
99.991%～99.999%, more preferably 99.993%～99.997%, most preferably 99.994%～99.996%；It is described
The colourity of ethylene carbonate product is preferably smaller than equal to 5, more preferably 1～5, more preferably 2～5, most preferably 3～4；It is described
The total content of the ethylene glycol and diethylene glycol of ethylene carbonate product is preferably smaller than equal to 30ppm, more preferably 5～25ppm, optimum
Elect 10～20ppm as；The water content of the ethylene carbonate product is preferably smaller than equal to 20ppm, more preferably 5～20ppm, most
Preferably 10～15ppm.
Step 2 of the present invention) can also be specially：
From the material of ethylene carbonate continuous treating tower side take-off, i.e. step 1) carry in the middle of the ethylene carbonate that obtains
Sterling, is introduced into batch fractionating tower feed surge tank, then Jing pumps are delivered to batch fractionating tower reactor, begins to warm up intensification, sets up complete
Tower VLE.Tower top first carries out total reflux operation 1～5 hour, and after the enrichment of tower top light component fraction, tower top starts to produce light group
Point, during tower top light component is gradually produced, to side line ethylene carbonate sample analysis, when sideline product purity reaches
99.99%, colourity be less than 5, it is aqueous less than 20ppm when, start produce LITHIUM BATTERY ethylene carbonate product.With batch fractionating
Carry out, sideline product purity is first raised and reduced afterwards, when product purity is less than LITHIUM BATTERY product quality indicator, stops extraction and produce
Product, after discharging tower reactor heavy constituent residual liquid, start next operation cycle.
Ethylene carbonate batch fractionating product tower of the present invention takes negative-pressure operation, tower top operating pressure to control in 1～5KPa,
Tower reactor operating pressure is controlled in 5～20KPa.Control interval rectifying column tower top operation temperature at 130～150 DEG C, grasp by control tower reactor
Make temperature at 135～170 DEG C.
The present invention is not particularly limited to the equipment of the batch fractionating technique, with interval well known to those skilled in the art
Rectifying column, those skilled in the art can be selected according to practical condition, raw material condition and product requirement and
Adjustment, refining effect of the present invention for further raising batch fractionating technique, batch fractionating tower of the present invention are preferably board-like
Tower or packed tower, more preferably packed tower.
The present invention is not particularly limited to the tower plate structure of the plate column, with plate column well known to those skilled in the art
Tower plate structure, those skilled in the art can be selected according to practical condition, raw material condition and product requirement
Select and adjust, tower plate structure of the present invention preferably includes bubble column, sieve-plate tower, valve tower or tongue shape tower.The present invention is to described
The form of bio-carrier of packed tower is not particularly limited, with the form of bio-carrier of packed tower well known to those skilled in the art, ability
Field technique personnel can be selected and be adjusted according to practical condition, raw material condition and product requirement, of the present invention
The form of bio-carrier of packed tower preferably includes structured packing or random packing, and more specifically preferably wire mesh packing, porcelain ripple are filled out
Material, metal corrugated packing, wooden-grid packing, Raschig ring, Pall ring, cascade ring, helical ring, ceramic ring, steel fill out circle, saddle type expect,
Quartz or glass spring, the present invention are the refining effect for further improving continuous rectificating technique, set with other of continuous rectifying tower
Phase matched combined is put, the continuous rectifying tower is preferably packed tower, more preferably wire mesh packing tower, most preferably rustless steel
Wire packing tower.
The present invention is not particularly limited to the parameter of the batch fractionating technique, with interval well known to those skilled in the art
Rectification process parameter, those skilled in the art can be carried out according to practical condition, raw material condition and product requirement
Select and adjust, refining effect of the present invention for further raising continuous rectificating technique, the tower of batch fractionating tower of the present invention
Plate number is preferably 30～60 pieces, more preferably 35～55 pieces, most preferably 40～50 pieces, is particularly preferred as 40 pieces；Institute of the present invention
The number of plates for stating batch fractionating tower side take-off is preferably the 15th～25th piece, more preferably the 17th～23rd piece, most preferably
19th～21st piece, it is particularly preferred as the 21st piece.Batch fractionating tower gating location of the present invention is preferably located at tower reactor,
That is tower reactor charging.
Sequence of the present invention to the column plate is not particularly limited, and knows conventional sort method with those skilled in the art
, i.e., it is the 1st block of column plate at tower top, is last 1 block of column plate at tower reactor.
Present invention also offers a kind of ethylene carbonate purification system, including：Continuous rectifying tower, continuous rectification column overhead are cold
Condenser, continuous rectifying tower overhead reflux device, continuous rectifying tower tower reactor reboiler, batch fractionating tower feeding buffer device, interval
Rectifying column, batch fractionating tower overhead condenser, batch fractionating tower overhead reflux device and batch fractionating tower tower reactor reboiler；
Described continuous rectifying tower overhead condenser one end is connected with continuous rectifying tower top gaseous phase outlet, the other end
It is connected with the continuous rectifying tower overhead reflux device, the continuous rectifying tower overhead reflux device and the continuous rectifying tower
Tower top fluid inlet is connected；
Described continuous rectifying tower tower reactor reboiler one end is connected with the continuous rectifying tower tower reactor liquid-phase outlet, the other end
It is connected with the continuous rectifying tower tower reactor gas phase import；
Described batch fractionating tower feeding buffer device one end is connected with the continuous rectifying tower survey line products export, another
End is connected with the batch fractionating tower charging aperture；
Described batch fractionating tower overhead condenser one end is connected with batch fractionating tower top gaseous phase outlet, the other end
It is connected with the batch fractionating tower overhead reflux device, the batch fractionating tower overhead reflux device and the batch fractionating tower
Tower top fluid inlet is connected；
Described batch fractionating tower tower reactor reboiler one end is connected with the continuous tower bottom of rectifying tower liquid-phase outlet of the interval, another
End is connected with the batch fractionating tower tower reactor gas phase import.
The present invention is not particularly limited to the continuous rectifying tower, with continuous rectifying tower well known to those skilled in the art is
Can, those skilled in the art can be selected and be adjusted according to practical condition, raw material condition and product requirement, this
The bright refining effect further to improve continuous rectifying tower, continuous rectifying tower of the present invention are preferably plate column or packed tower,
More preferably packed tower.
The present invention is not particularly limited to the tower plate structure of the plate column, with plate column well known to those skilled in the art
Tower plate structure, those skilled in the art can be selected according to practical condition, raw material condition and product requirement
Select and adjust, tower plate structure of the present invention preferably includes bubble column, sieve-plate tower, valve tower or tongue shape tower.The present invention is to described
The form of bio-carrier of packed tower is not particularly limited, with the form of bio-carrier of packed tower well known to those skilled in the art, ability
Field technique personnel can be selected and be adjusted according to practical condition, raw material condition and product requirement, of the present invention
The form of bio-carrier of packed tower preferably includes structured packing or random packing, and more specifically preferably wire mesh packing, porcelain ripple are filled out
Material, metal corrugated packing, wooden-grid packing, Raschig ring, Pall ring, cascade ring, helical ring, ceramic ring, steel fill out circle, saddle type expect,
Quartz or glass spring, the present invention are the refining effect for further improving continuous rectifying tower, arrange with other of continuous rectifying tower
Phase matched combined, the continuous rectifying tower are preferably packed tower, more preferably wire mesh packing tower, most preferably stainless steel silk
Net packed tower.
The present invention is not particularly limited to the structural parameters of the continuous rectifying tower, with company well known to those skilled in the art
The structural parameters of continuous rectifying column, those skilled in the art can be wanted according to practical condition, raw material condition and product
Ask and selected and adjusted, refining effect of the present invention for further raising continuous rectifying tower, continuous rectifying tower of the present invention
The number of plates be preferably 30～60 pieces, more preferably 35～55 pieces, most preferably 40～50 pieces, be particularly preferred as 40 pieces；This
The number of plates of the side entry feed mouth position of the bright continuous rectifying tower is preferably the 25th～35th piece, and the more preferably the 27th～the 33rd
Block, is particularly preferred as the 31st piece by most preferably the 29th～31st piece；The products export position of continuous rectifying tower of the present invention,
I.e. the number of plates of side take-off is preferably the 5th～15th piece, more preferably the 7th～13rd piece, most preferably the 9th～11st piece,
It is particularly preferred as the 11st piece.
Continuous rectifying tower overhead reflux device of the present invention is connected with the continuous rectifying tower tower top fluid inlet, institute
State the 1st block of column plate that the position being connected is preferably the continuous rectifying tower.
Sequence of the present invention to the column plate is not particularly limited, and knows conventional sort method with those skilled in the art
, i.e., it is the 1st block of column plate at tower top, is last 1 block of column plate at tower reactor.
Sequence of the present invention to the column plate is not particularly limited, and knows conventional sort method with those skilled in the art
, i.e., it is the 1st block of column plate at tower top, is last 1 block of column plate at tower reactor.The model of the number of plates of outlet of the present invention or import
Enclose value be preferably all or relation, i.e., in the range of carry out selecting a selection.
The present invention is not particularly limited to the equipment of the batch fractionating tower, with interval well known to those skilled in the art essence
Tower is evaporated, those skilled in the art can be selected and be adjusted according to practical condition, raw material condition and product requirement
Whole, refining effect of the present invention for further raising batch fractionating technique, batch fractionating tower of the present invention are preferably plate column
Or packed tower, more preferably packed tower.
The present invention is not particularly limited to the tower plate structure of the plate column, with plate column well known to those skilled in the art
Tower plate structure, those skilled in the art can be selected according to practical condition, raw material condition and product requirement
Select and adjust, tower plate structure of the present invention preferably includes bubble column, sieve-plate tower, valve tower or tongue shape tower.The present invention is to described
The form of bio-carrier of packed tower is not particularly limited, with the form of bio-carrier of packed tower well known to those skilled in the art, ability
Field technique personnel can be selected and be adjusted according to practical condition, raw material condition and product requirement, of the present invention
The form of bio-carrier of packed tower preferably includes structured packing or random packing, and more specifically preferably wire mesh packing, porcelain ripple are filled out
Material, metal corrugated packing, wooden-grid packing, Raschig ring, Pall ring, cascade ring, helical ring, ceramic ring, steel fill out circle, saddle type expect,
Quartz or glass spring, the present invention are the refining effect for further improving continuous rectificating technique, set with other of continuous rectifying tower
Phase matched combined is put, the continuous rectifying tower is preferably packed tower, more preferably wire mesh packing tower, most preferably rustless steel
Wire packing tower.
The present invention is not particularly limited to the structural parameters of the batch fractionating tower, with well known to those skilled in the art
Have a rest the structural parameters of rectifying column, those skilled in the art can will according to practical condition, raw material condition and product
Ask and selected and adjusted, refining effect of the present invention for further raising continuous rectifying tower, batch fractionating tower of the present invention
The number of plates be preferably 30～60 pieces, more preferably 35～55 pieces, most preferably 40～50 pieces, be particularly preferred as 40 pieces；This
The products export position of the bright batch fractionating tower, the i.e. number of plates of side take-off are preferably the 15th～25th piece, more preferably
17th～23rd piece, most preferably the 19th～21st piece, it is particularly preferred as the 21st piece.Batch fractionating tower charging aperture of the present invention
Position is preferably located at tower reactor, i.e. tower reactor charging.
Above-mentioned steps of the present invention provide a kind of ethylene carbonate purifying technique and purification system, and the present invention is overcoming now
There is the cyclic carbonate of industrialized production present in technology, the technology prejudice of continuous rectification operation can not be used in purification
On the basis of, combined using continuous rectification operation and batch fractionating operation, Creative Design is carried out on overall purifying technique, will
Thick ethylene carbonate material, refined through continuous treating tower, tower top, bottom of towe produce weight composition impurity, side take-off carbon respectively
Vinyl acetate material, enters back into batch fractionating tower and further refines, and after batch fractionating tower overhead extraction light component impurity, finally exists
Side take-off ethylene carbonate product.Test result indicate that, the ethylene carbonate after present invention purification, purity are higher than 99.99%,
It is aqueous less than 20ppm, colourity is less than 5, and ethylene glycol and diethylene glycol total content are less than 30ppm, and indices fully meet lithium ion
The index request of battery electrolyte solvent application.
In order to further illustrate the present invention, a kind of ethylene carbonate purification work that with reference to embodiments present invention is provided
Skill and deduction system are described in detail, but it is to be understood that these embodiments are under premised on technical solution of the present invention
Implemented, given detailed embodiment and specific operating process, simply for further illustrate the present invention feature and
Advantage, rather than limiting to the claimed invention, protection scope of the present invention are also not necessarily limited to following embodiments.
Embodiment 1
The technological process sketch plan of the ethylene carbonate purifying technique provided for the present invention referring to Fig. 1, Fig. 1.Wherein, 1 is carbon
Vinyl acetate continuous rectifying tower, 2 is continuous rectifying tower overhead condenser, and 3 is continuous rectifying tower return tank of top of the tower, and 4 are interval essence
Tower feed surge tank is evaporated, 5 is continuous rectifying tower tower reactor reboiler, and 6 is ethylene carbonate batch fractionating tower, and 7 is batch fractionating tower
Overhead condenser, 8 is batch fractionating tower return tank of top of the tower, and 9 is batch fractionating tower tower reactor reboiler.
The present embodiment is adopted with oxirane and carbon dioxide as raw material, and compound ion liquid is the purity of catalyst synthesis
Ethylene carbonate for 99.83% is raw material.
In the present embodiment, ethylene carbonate continuous rectifying tower adopts BX stainless steel cloth fillers, totally four layers of filler, and per layer is filled out
Material height is 4 meters, and theoretical cam curve is 48 blocks of column plates, and between three, four layers of filler, theoretical cam curve is for feedstock position
25 blocks of theoretical trays, between one, two layers of filler, theoretical cam curve is the 13rd block of theoretical tray to unloading position.
Batch fractionating tower adopts BX stainless steel cloth fillers, totally four layers of filler, and every layer of packed height is 4 meters, theoretical tray
Number for 48 blocks of column plates, feedstock position in tower reactor, side take-off product space between one, two layers of filler, theoretical cam curve
For the 13rd piece of theoretical plate.
(1) step 1：Ethylene carbonate crude product is delivered to into ethylene carbonate continuous rectifying tower with the flow of 1500kg/h,
Overhead extraction light component flow is 100kg/h, and tower reactor extraction restructuring shunt volume is 100kg/h, side take-off 1300kg/h's
99.93% ethylene carbonate product is delivered to ethylene carbonate batch fractionating tower feed surge tank.
The operating condition of the continuous rectifying tower is that overhead reflux amount is 2000kg/h, and tower top operating pressure is 3KPa, is operated
Temperature is 138 DEG C, and tower reactor operating pressure is 9KPa, and operation temperature is 149 DEG C.
(2) step 2：Ethylene carbonate material Jing pumps from batch fractionating tower feed surge tank are delivered to batch fractionating tower
18 tons of tower reactor, tower reactor reboiler begin to warm up intensification and begin setting up full tower VLE, and tower top is taken total reflux operation, controlled back
Flow is 6000kg/h, and after total reflux operation 1.5 hours, tower top starts to produce light component material, overhead extraction light component material
Flow-control after extraction light component operates 2 hours, is opened side take-off mouth sample analysis, works as purity assay in 1300kg/h
Higher than 99.99%, colourity is less than 5, aqueous to start extraction when being less than 30ppm and close less than 20ppm, ethylene glycol and diethylene glycol total content
Lattice LITHIUM BATTERY ethylene carbonate product.Product extraction during every half an hour sample analysis ethylene carbonate product purity,
The index such as aqueous, the purity of product first rise, and highest purity reaches 99.995%, then begins to decline, when side line ethylene carbonate
When the purity of ester product is reduced to 99.99%, stop product extraction, after discharging kettle material, start the next operation cycle.Side
The flow of overhead extraction light component is turned down during line extraction product gradually.In this example batch fractionating operation cycle, side line is adopted altogether
Go out 13.2 tons of the product that purity meets LITHIUM BATTERY ethylene carbonate quality index.The tower operating condition for tower top operating pressure is
4KPa, 138～142 DEG C of tower top operation temperature, tower reactor operating pressure 12KPa, 146～154 DEG C of tower reactor operation temperature.
Purity is 99.992% to be detected to ethylene carbonate product prepared by the embodiment of the present invention 1, colourity is less than 5,
The total content of ethylene glycol and diethylene glycol is 18ppm, and water content is 16ppm.
Embodiment 2
It is raw material that the present embodiment adopts purity for 99.74% ethylene carbonate.
In the present embodiment, ethylene carbonate continuous rectifying tower adopts BX stainless steel cloth fillers, totally four layers of filler, and per layer is filled out
Material height is 4 meters, and theoretical cam curve is 48 blocks of column plates, and between three, four layers of filler, theoretical cam curve is for feedstock position
25 blocks of theoretical trays, between one, two layers of filler, theoretical cam curve is the 13rd block of theoretical tray to unloading position.
Batch fractionating tower adopts BX stainless steel cloth fillers, totally four layers of filler, and every layer of packed height is 4 meters, theoretical tray
Number for 48 blocks of column plates, feedstock position in tower reactor, side take-off product space between one, two layers of filler, theoretical cam curve
For the 13rd piece of theoretical plate.
(1) step 1：Ethylene carbonate crude product is delivered to into ethylene carbonate continuous rectifying tower with the flow of 1500kg/h,
Overhead extraction light component flow is 130kg/h, and tower reactor extraction restructuring shunt volume is 160kg/h, side take-off 1210kg/h's
99.95% ethylene carbonate product is delivered to ethylene carbonate batch fractionating tower feed surge tank.
The operating condition of the continuous rectifying tower is that overhead reflux amount is 2300kg/h, and tower top operating pressure is 2KPa, is operated
Temperature is 135 DEG C, and tower reactor operating pressure is 9KPa, and operation temperature is 150 DEG C.
(2) step 2：Ethylene carbonate material Jing pumps from batch fractionating tower feed surge tank are delivered to batch fractionating tower
18 tons of tower reactor, tower reactor reboiler begin to warm up intensification and begin setting up full tower VLE, and tower top is taken total reflux operation, controlled back
Flow is 5500kg/h, and after total reflux operation 2 hours, tower top starts to produce light component material, overhead extraction light component material stream
Control is measured in 1500kg/h, after extraction light component operates 2 hours, side take-off mouth sample analysis is opened, when purity assay height
In 99.99%, colourity is less than 5, aqueous less than 20ppm, and ethylene glycol and diethylene glycol total content start extraction when being less than 30ppm qualified
LITHIUM BATTERY ethylene carbonate product.Product extraction during every half an hour sample analysis ethylene carbonate product purity, contain
The indexs such as water, the purity of product first rise, and highest purity reaches 99.997%, then begins to decline, when side line ethylene carbonate
When the purity of product is reduced to 99.99%, stop product extraction, after discharging kettle material, start the next operation cycle.Side line
The flow of overhead extraction light component is turned down during extraction product gradually.In this example batch fractionating operation cycle, side line is produced altogether
Purity meets 12.2 tons of the product of LITHIUM BATTERY ethylene carbonate quality index.The tower operating condition for tower top operating pressure is
2KPa, 135～141 DEG C of tower top operation temperature, tower reactor operating pressure 10KPa, 145～153 DEG C of tower reactor operation temperature.
Purity is 99.993% to be detected to ethylene carbonate product prepared by the embodiment of the present invention 2, colourity is less than 5,
The total content of ethylene glycol and diethylene glycol is 23ppm, and water content is 12ppm.
Embodiment 3
It is raw material that the present embodiment adopts purity for 99.57% ethylene carbonate.
In the present embodiment, ethylene carbonate continuous rectifying tower adopts BX stainless steel cloth fillers, totally four layers of filler, and per layer is filled out
Material height is 4 meters, and theoretical cam curve is 48 blocks of column plates, and between three, four layers of filler, theoretical cam curve is for feedstock position
25 blocks of theoretical trays, between one, two layers of filler, theoretical cam curve is the 13rd block of theoretical tray to unloading position.
Batch fractionating tower adopts BX stainless steel cloth fillers, totally four layers of filler, and every layer of packed height is 4 meters, theoretical tray
Number for 48 blocks of column plates, feedstock position in tower reactor, side take-off product space between one, two layers of filler, theoretical cam curve
For the 13rd piece of theoretical plate.
(1) step 1：Ethylene carbonate crude product is delivered to into ethylene carbonate continuous rectifying tower with the flow of 1500kg/h,
Overhead extraction light component flow is 160kg/h, and tower reactor extraction restructuring shunt volume is 180kg/h, side take-off 1160kg/h's
99.95% ethylene carbonate product is delivered to ethylene carbonate batch fractionating tower feed surge tank.
The operating condition of the continuous rectifying tower is that overhead reflux amount is 2500kg/h, and tower top operating pressure is 2KPa, is operated
Temperature is 133 DEG C, and tower reactor operating pressure is 10KPa, and operation temperature is 152 DEG C.
(2) step 2：Ethylene carbonate material Jing pumps from batch fractionating tower feed surge tank are delivered to batch fractionating tower
18 tons of tower reactor, tower reactor reboiler begin to warm up intensification and begin setting up full tower VLE, and tower top is taken total reflux operation, controlled back
Flow is 5500kg/h, and after total reflux operation 2 hours, tower top starts to produce light component material, overhead extraction light component material stream
Amount control after extraction light component operates 1.5 hours, is opened side take-off mouth sample analysis, works as purity assay in 2000kg/h
Higher than 99.99%, colourity is less than 5, aqueous to start extraction when being less than 30ppm and close less than 20ppm, ethylene glycol and diethylene glycol total content
Lattice LITHIUM BATTERY ethylene carbonate product.Product extraction during every half an hour sample analysis ethylene carbonate product purity,
The index such as aqueous, the purity of product first rise, and highest purity reaches 99.994%, then begins to decline, when side line ethylene carbonate
When the purity of ester product is reduced to 99.99%, stop product extraction, after discharging kettle material, start the next operation cycle.Side
The flow of overhead extraction light component is turned down during line extraction product gradually.In this example batch fractionating operation cycle, side line is adopted altogether
Go out 11.8 tons of the product that purity meets LITHIUM BATTERY ethylene carbonate quality index.The tower operating condition for tower top operating pressure is
2KPa, 133～142 DEG C of tower top operation temperature, tower reactor operating pressure 9KPa, 144～155 DEG C of tower reactor operation temperature.
To the embodiment of the present invention 3 prepare ethylene carbonate product detect that purity is 99.992%, colourity be less than
5, the total content of ethylene glycol and diethylene glycol is 26ppm, and water content is 13ppm.
A kind of highly purified ethylene carbonate purifying technique and deduction system for providing to the present invention above has been carried out in detail
Introduction, specific case used herein is set forth to the principle and embodiment of the present invention, and above example is said
It is bright to be only intended to help and understand the method for the present invention and its core concept, including best mode, and also cause appointing for this area
What technical staff can put into practice the present invention.It should be pointed out that for those skilled in the art, without departing from
On the premise of the principle of the invention, some improvement and modification can also be carried out to the present invention, these improve and modification also falls into this
In bright scope of the claims.The scope of patent protection of the present invention is defined by the claims, and may include this area
Technical staff it is conceivable that other embodiment.If these other embodiments have is not different from claim character express
Structural element, or if they include equivalent structural elements of the character express without essence difference with claim, then
These other embodiments also should be comprising within the scope of the claims.
Claims (10)
1. a kind of ethylene carbonate purifying technique, it is characterised in that comprise the following steps：
1) ethylene carbonate crude product is sent into into continuous rectificating technique, top removing light component impurity, bottom remove heavy constituent impurity,
Side take-off ethylene carbonate intermediate purification product；
2) after the ethylene carbonate intermediate purification product that obtain above-mentioned steps are buffered, batch fractionating technique is sent into, heating is set up
Top removing light component material, side take-off ethylene carbonate product after vapor liquid equilibrium.
2. purifying technique according to claim 1, it is characterised in that the step 1) in, the operating pressure at the top
For 1～5KPa, the operation temperature at the top is 130～150 DEG C；The operating pressure of the bottom be 5～20KPa, the bottom
The operation temperature in portion is 135～165 DEG C；
The step 2) in, the operating pressure at the top is 1～5KPa, and the operation temperature at the top is 130～150 DEG C；
The operating pressure of the bottom is 5～20KPa, and the operation temperature of the bottom is 135～170 DEG C.
3. purifying technique according to claim 2, it is characterised in that the purity of the ethylene carbonate crude product is 99.5%
～99.8%；
The purity of the ethylene carbonate intermediate purification product is 99.9%～99.98%.
4. the purifying technique according to claims 1 to 3 any one, it is characterised in that the step 1) in, the top
Removing light component impurity is specially top and carries out condensing reflux removing light component impurity；
The reflux ratio of the backflow is 20～80；
The produced quantity of the light component impurity is 0.1～0.4 with the ratio of the inlet amount of the ethylene carbonate crude product；
The bottom removing heavy constituent impurity is specially bottom and is boiled circularly removing heavy constituent impurity again；
The produced quantity of the heavy constituent impurity is 0.1～0.4 with the ratio of the inlet amount of the ethylene carbonate crude product.
5. purifying technique according to claim 1, it is characterised in that the step 2) it is specially：
21), after the ethylene carbonate intermediate purification product that obtain above-mentioned steps are buffered, send into batch fractionating technique；
22), after vapor liquid equilibrium is set up in heating, top carries out total reflux operation, and bottom is boiled extinction recycle operation again；
23) at the top of, light component material collection removes light component material to after finite concentration, first, and side line starts to produce ethylene carbonate again
Ester product；
24) ethylene carbonate product discharges bottom heavy constituent residual liquid less than extraction ethylene carbonate after standard, is stopped；
25) circulation step 22)～24).
6. purifying technique according to claim 5, it is characterised in that the step 23) in, the side line starts to produce carbon
After vinyl acetate product, the removing amount of top light component material is gradually reduced.
7. purifying technique according to claim 5, it is characterised in that having for top with reference to condition for the vapor liquid equilibrium evaporates
Go out thing, begin with backflow；
The temperature of the heating is 130～160 DEG C；
The time of the total reflux operation is 1～5 hour；
The time for first removing light component material is 0.5～3 hour；
The removing amount of the light component material is 0.1～0.3 with the ratio of the inlet amount for sending into batch fractionating technique.
8. purifying technique according to claim 5, it is characterised in that the light component material collection is light to finite concentration
Constituent content is in 0.1～2wt%；
During the standard of the ethylene carbonate product includes the total content and water content of purity, colourity, ethylene glycol and diethylene glycol
One or more.
9. the purifying technique according to claim 5～8 any one, it is characterised in that the ethylene carbonate product
Purity is more than or equal to 99.99%；
The colourity of the ethylene carbonate product is less than or equal to 5；
The total content of the ethylene glycol and diethylene glycol of the ethylene carbonate product is less than or equal to 30ppm；
The water content of the ethylene carbonate product is less than or equal to 20ppm.
10. a kind of ethylene carbonate purification system, it is characterised in that include：Continuous rectifying tower, continuous rectifying tower overhead condensation
Device, continuous rectifying tower overhead reflux device, continuous rectifying tower tower reactor reboiler, batch fractionating tower feeding buffer device, interval essence
Evaporate tower, batch fractionating tower overhead condenser, batch fractionating tower overhead reflux device and batch fractionating tower tower reactor reboiler；
The outlet of described continuous rectifying tower overhead condenser one end and the continuous rectifying tower top gaseous phase is connected, the other end and institute
State continuous rectifying tower overhead reflux device to be connected, the continuous rectifying tower overhead reflux device and the continuous rectification column overhead
Fluid inlet is connected；
Described continuous rectifying tower tower reactor reboiler one end is connected with the continuous rectifying tower tower reactor liquid-phase outlet, the other end and institute
State continuous rectifying tower tower reactor gas phase import to be connected；
Described batch fractionating tower feeding buffer device one end is connected with the continuous rectifying tower survey line products export, the other end with
The batch fractionating tower charging aperture is connected；
The outlet of described batch fractionating tower overhead condenser one end and the batch fractionating tower top gaseous phase is connected, the other end and institute
State batch fractionating tower overhead reflux device to be connected, the batch fractionating tower overhead reflux device and the batch fractionating column overhead
Fluid inlet is connected；
The continuous tower bottom of rectifying tower liquid-phase outlet of described batch fractionating tower tower reactor reboiler one end and the interval is connected, the other end with
The batch fractionating tower tower reactor gas phase import is connected.
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|---|---|---|---|---|
| CN107501230A (en) * | 2017-09-29 | 2017-12-22 | 福州大学 | Crystallization couples the device and method for preparing electron level ethylene carbonate with rectifying |
| CN107915662A (en) * | 2017-12-20 | 2018-04-17 | 青岛科技大学 | Separation, the device and method of purification m-xylylene diisocyanate |
| CN108440489A (en) * | 2018-05-25 | 2018-08-24 | 辽宁港隆化工有限公司 | A kind of crystallization apparatus and purification process for the refined purification of ethylene carbonate |
| CN111100003A (en) * | 2018-10-25 | 2020-05-05 | 中国石油化工股份有限公司 | Crystallization purification process of high-purity ethylene carbonate |
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| CN114011101A (en) * | 2021-04-08 | 2022-02-08 | 旭化成株式会社 | Industrial process for producing cyclic alkylene carbonate |
| WO2022215297A1 (en) | 2021-04-08 | 2022-10-13 | 旭化成株式会社 | Industrial production method of cyclic alkylene carbonate |
| EP4321510A4 (en) * | 2021-04-08 | 2024-10-16 | Asahi Kasei Kk | Industrial production method of cyclic alkylene carbonate |
| CN113559804A (en) * | 2021-09-22 | 2021-10-29 | 山东海科新源材料科技股份有限公司 | Vinylene carbonate manufacturing equipment |
| CN116023236A (en) * | 2021-10-26 | 2023-04-28 | 中国石油化工股份有限公司 | Purification method, purification system and application of crude ethylene glycol |
| CN114369080A (en) * | 2022-01-19 | 2022-04-19 | 凯瑞环保科技股份有限公司 | Device and method for synthesizing ethylene carbonate or propylene carbonate |
| CN114437014A (en) * | 2022-01-19 | 2022-05-06 | 凯瑞环保科技股份有限公司 | Device and method for synthesizing ethylene carbonate or propylene carbonate |
| CN114437014B (en) * | 2022-01-19 | 2024-03-19 | 凯瑞环保科技股份有限公司 | Device and method for synthesizing ethylene carbonate or propylene carbonate |
| CN115043713A (en) * | 2022-06-27 | 2022-09-13 | 山东海科新源材料科技股份有限公司 | Diethylene glycol purification device and method |
| CN115043713B (en) * | 2022-06-27 | 2023-08-08 | 山东海科新源材料科技股份有限公司 | Diethylene glycol purifying device and method |
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